Single-Chip Dynamic Nuclear Polarization Microsystem

Integration of the sensitivity-relevant electronics of nuclear magnetic resonance (NMR) and electron spin resonance (ESR) spectrometers on a single chip is a promising approach to improve the limit of detection, especially for samples in the nanoliter and subnanoliter range. Here, we demonstrate the cointegration on a single silicon chip of the front-end electronics of NMR and ESR detectors. Nergiz Sahin Solmaz, a PhD student at LMIS1, combined the single-chip NMR detector designed by Marco Grisi and the single-chip ESR detector designed by Alessandro V. Matheoud, two former PhD students of LMIS1. The excitation/detection planar spiral microcoils of the NMR and ESR detectors are concentric and interrogate the same sample volume. This combination of sensors allows one to perform dynamic nuclear polarization (DNP) experiments using a single-chip-integrated microsystem having an area of about 2 mm². In particular, we report ¹H DNP-enhanced NMR experiments on liquid samples having a volume of about 1 nL performed at 10.7 GHz(ESR)/16 MHz(NMR). NMR enhancements as large as 50 are achieved on TEMPOL/H₂O solutions at room temperature. The use of state-of-the-art submicrometer integrated circuit technologies should allow the future extension of the single-chip DNP microsystem approach proposed here up the THz(ESR)/GHz(NMR) region, corresponding to the strongest static magnetic fields currently available. Particularly interesting is the possibility to create arrays of such sensors for parallel DNP-enhanced NMR spectroscopy of nanoliter and subnanoliter samples.

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https://pubs.acs.org/doi/10.1021/acs.analchem.0c01221